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利用反相高效液相色谱法从赤泥中分离钪和稀土元素的研究。

Investigation of the separation of scandium and rare earth elements from red mud by use of reversed-phase HPLC.

作者信息

Tsakanika Lambrini V, Ochsenkühn-Petropoulou Maria Th, Mendrinos Leonidas N

机构信息

School of Chemical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 15773 Athens, Greece.

出版信息

Anal Bioanal Chem. 2004 Jul;379(5-6):796-802. doi: 10.1007/s00216-004-2667-1. Epub 2004 Jun 18.

Abstract

A chromatographic method has been developed for separation and determination of scandium (Sc) and rare earth elements (REEs) in samples from a red mud (RM)-utilization process. Reversed-phase high-performance liquid chromatography (RP-HPLC) with post-column derivatization using 4-(2-pyridylazo)-resorcinol (PAR) and UV-visible detection at 520 nm was tested using different gradient elution profiles and pH values to optimize separation and recovery, primarily for Sc but also for yttrium and the individual lanthanides, from iron present in the samples. The separation was performed in less than 20 min by use of a mobile phase gradient. The concentration of alpha-hydroxyisobutyric acid ( alpha-HIBA), as eluent, was altered from 0.06 to 0.4 mol L(-1) (pH 3.7) and 0.01 mol L(-1) sodium salt n-octane sulfonic acid (OS) was used as modifier. Very low detection limits in the nanogram range and a good resolution for Sc and REEs except for Y/Dy were achieved. Before application of the method to the red mud samples and to the corresponding bauxites, Sc and REEs were leached from red mud with 0.6 mol L(-1) HNO(3) and mostly separated, as a group, from the main elements by ion exchange/selective elution (6 mol L(-1) HNO(3)) in accordance with a pilot-plant process developed in this laboratory. After evaporation of the eluent to dryness the extracted elements were re-dissolved in the mobile phase. By use of this chromatographic method Sc, which is the most expensive of the elements investigated and occurs in economically interesting concentrations in red mud, could be separated not only from co-existing Fe but also from Y/Dy, Yb, Er, Ho, Gd, Eu, Sm, Nd, Pr, Ce and La. All the elements investigated were individually recovered. Their recoveries were found to be nearly quantitative.

摘要

已开发出一种色谱方法,用于分离和测定赤泥(RM)利用过程中样品中的钪(Sc)和稀土元素(REEs)。采用反相高效液相色谱(RP-HPLC),柱后衍生使用4-(2-吡啶偶氮)-间苯二酚(PAR),并在520nm处进行紫外-可见检测,通过测试不同的梯度洗脱曲线和pH值来优化分离和回收率,主要针对Sc,也包括钇和各个镧系元素,以从样品中的铁中分离出来。使用流动相梯度在不到20分钟内完成分离。作为洗脱剂的α-羟基异丁酸(α-HIBA)浓度从0.06改变为0.4mol L(-1)(pH 3.7),并使用0.01mol L(-1)的正辛烷磺酸钠盐(OS)作为改性剂。实现了纳克范围内的极低检测限以及除Y/Dy外Sc和REEs的良好分离度。在将该方法应用于赤泥样品和相应的铝土矿之前,用0.6mol L(-1) HNO(3)从赤泥中浸出Sc和REEs,并根据本实验室开发的中试工艺,通过离子交换/选择性洗脱(6mol L(-1) HNO(3))将它们作为一组与主要元素大部分分离。洗脱剂蒸发至干后,将提取的元素重新溶解在流动相中。通过使用这种色谱方法,Sc作为所研究元素中最昂贵的元素,且在赤泥中以具有经济意义的浓度存在,不仅可以与共存的Fe分离,还可以与Y/Dy、Yb、Er、Ho、Gd、Eu、Sm、Nd、Pr、Ce和La分离。所有研究的元素都能单独回收。发现它们的回收率几乎是定量的。

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